Hydrogen Peroxide → 3,4,5-Trichloropyridine N-oxide

To a stirred solution of 3,4,5-trichloropyridine (1 g, 5.45 mmol) in dichloromethane (20 mL) at 0° C., was added dropwise a 30% hydrogen peroxide solution (1.2 mL, 10.9 mmol). Following the addition, the temperature was allowed to rise to room temperature and was stirred for 15 hours. The reaction mixture was diluted with dichloromethane (50 mL) and was washed with water (10 mL) and then by brine (25 mL×2). The organic phase was dried (Na2SO4), concentrated under vacuum to afford the title product as a white solid (0.8 g, 74% yield). 1H NMR (400 MHz, d6-DMSO) δ: 8.78 (2H, s). MS m/z: 197.90 [M+H]+.

1. additionthe addition
2. customto rise to room temperature
3. washwas washed with water (10 mL)
4. dry with materialThe organic phase was dried (Na2SO4)
5. concentrationconcentrated under vacuum

ORD record

ord-2c10a1e6a80b4647b1bb3f8af069cc5d

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08680139B2